Process of making ammonia.



C. KRAUSS.

PROCESS OP MAKING AMMONIA.

APPLICATION FILED MAY 24, 1907. BENBWED MAR. 31,1909.

Patented May 18, 1909.

Elgin ymwy amaransrarns nagaan carica OONSTANTIN KBIlUSS, OF WESTEREGELN, GERMANY, ASSIGNOR TO GESELLSHAFT FR STIGKSTOFFDUNGER, GESELLSCHAFT MIT BESCHRNKTER HAFTUNG, OF WESTERE- GELN, GERMANY.

Patented may 18,1909.

Application med lay 91, 1907, Serial No. 875,396. Renewed March 31, 1909. Serial No. 487,052.

i T o all whom it may concern.'

Be it known that l, CONSTANTIN KnAUss,

of lVesteregeln, Germany, have invented a certain new and useful Process of Making Ammonia, or Which the following is a specication.

lt is a Well known fact that by the reaction of Water on cyanids and cyanamids, as for instance cyanid of potassium, cyanid of calcium, cyanid of sodium, the nitrogen of these compounds may be converted into ammonia. It is furthermore known that the nitrogen of such com ounds as are obtained by the reaction o nitrogen upon carbids or carbid-forming mixtures at high tem leratures may be converted into ammonia y Waterand heat. Practice has shown that, when pure Water (or steam) is used in the said process, the reaction proceeds but very slowly, Whether the nitrogen comounds are `made use of in pieces or in the orm oa powder, and by using' pure Water the reaction cannot be .carried out quantitatively. For these reasons4 it is hardly possible to use this reaction directl as a commercial rocess. I have found y experiment an practical use, that by reacting `upon the said nitrogen compounds with Wa- -ter (or steam) and heat in the chlorid of calcium, the whole o the nitro gen of these compounds can be converted into ammonia, and this very easily and in a comparatively short time.

My said invention is fully shown and described in' the following specification of which the accompanying draw-ving forms a part wherein similar letters of reference designate like or equivalent arts Wherever found' throughout the severa views and in which- Figure 1 is onc form of my improved aparatus for carrying my improved process into eflect, and Fig. 2 is a like view-of a modied form of apparatus for the same urpose. Referring to the drawing: As s own in Fig. 1, the reference letter M designates a inutile closed on all sides and heated from the re-place F underneath, said mullie being provided with an o ening O for charging and discharging an With an outlet A at the top for the ammonia developed. In said Inutile is placed a charge of i'inely pulverized calcium c anid intimately mixed With about the doulile of its weight of a conconstant.

resence of centrated `aqueous solution of chlorid of calcium the opening O isv vthan hermetically closed and the mufle heated. The temperature of the reaction mass will then quickly rise to over 100 degrees C., and ammonia, gas and vapors will escape from the mullfle which are condensed in suitable condensing receptacles not shown. On further heating the tem erature will gradually rise, the formation o ammonia remaining nearly After some hours the development of ammonia Will decrease, the temperature is then caused to rise quickly to over 25()v degrees C. Up to this moment two thirds of the Whole nitrogen will have been converted into ammonia. When the ammonia will again begin to develop, and

the last third of nitrogen contained in the `mass nia.

will be distilled in the form of ammo As soon as the temperature shall have reached 4G() degrees, it will be found the Whole of the nitrogen has been converted into ammonia. ln order to drive out the last of nitrogen, Wet steam is allowed to flow into the muflle through a suitable pipe P located at any convenient point.A he llatter is then opened, the grayv residue removed,

and the operation repeated. Such an operation will generally take l5 to2() hours according to the thickness of the layer ol material employed. Any pulverizing of the substance may be prevented by reducing the nitro' en compounds to egg-slzed pieces, thoroug y saturating these pieces with a concentrated aqueous solution of chlorid of calcium and subjecting them to the above Idescribed process.

-For carrying out the process continuously, l make use ofthe a paratus shown in Fig. 2, and the process is then carried out in the following manner: Pieces of calcium cyanamid of the 'size or from a Walnut to an eg are thoroughly saturated with a solution o concentrated chlorid of calcium. Such im reg'- nated pieces are then put into the cylin er or muflle C, Which has at its top a funnel-sha ed enlargement or hopper E, provided Wit a valve-obturator K; at the bottom ofthe cylinder is a rotating grate R with an obturable ash-pit B for receiving the residue or ashes, While the gaseous products of combustion from the grate F, ass 9H byway of a :flue or lues L. From t 's ash-pit the ammonia produced is sucked off by means of a fan [rial with chlorid of calcium to the action of through the pipe A. The upright cylinder or muille C is built into a brickwork chamber, and is heated usually by means of a nre-place G. The vapors of ammonia and Water developed are drawn oi through the mass in the direction shown by the arrows. The

residues freed from nitrogen are caused to` fall through the grate into the ash-pit at intervals and are removed therefrom from time to time, and the cylinder is in like manner d With new material through the hop- Ii Taking cyanamid of calcium as an example ofthe chemical to be treated, it is probable that the following reaction takes place v1z:

chlorid of calcium, then adding the Water required and heating the Whole, and that the process may also be carried out by mixing the nitrogen compounds With chlorid of calcium, and causing steam and heat to react upon the mixture, and I do not intend to limit my invention in all its details to the exact manner of carrying the same into eiiect hereinbefore described, nor to either of the j forms of apparatusshoWn but Having now fully described my invention, what I claim as new and desire to secure by Letters Patent is 1. The process of producing ammonia from suitable cyanogcn compounds which consist in subjecting a mixture of the same With chlorid of calcium to the action of Water and heat. I l

2. The process of producing ammonia from cyanamids, which consists in subjecting a mixture of cyanamids with chlorid of calcium to the action of Water and heat.

3. The process of reducing ammonia from calcium-cyanamid), which consists in subjecting a mixture of calcium cyanamid With chlorid of calcium to the action of Water and heat.

4. The process of producing ammonia from suitable cyanogcn compounds which conslsts 1n subjecting a mixture ofthe matestcam and heat.

5. The process of producing ammonia from cyanamids, which consists in subjecting a mixture of cyanamids Withchlorid of calcium to the action of steam and heat.

6. The process of roducing ammonia from calcium-cyanami which consists in subjecting a mixture of calcium-cyanamid with chlorid of calcium to the action of steam and heat..

7. The process of producing ammonia from suitable cyanogcn compounds which consists in mixing the material With an aqueous solution of chlorid of calcium and subjecting the mixture to the action of heat.

8. The process of producing ammonia from cyanamids which consists in mixing the cyanamids with an aqueous solution of chlorid of calcium and subjecting the mixture to the action of heat.

9. The process of producing ammonia from calcium cyanamid, which consists in mixing the calciumcyanamid with an aqueous solution of chlorid of calcium and subjecting the mixture to the action of heat.

10. The process of producing ammonia from suitable cyanogcn compounds which consists in reducing the material to suitably sized pieces, saturating the same with a concentrated aqueous solution of chlorid of calcium and subjecting the same to heat.

11. The process of producing ammonia tion of chlorid of calcium and subjecting the same to heat.

12. The rocess \of producing ammonia from suitab e cyanogcn. compounds which consists in adding thereto disintegrated chlo- 1 rid of calcium and subjecting the mixture to the action of Water and heat.

13. The process of producing ammonia from suitable cyanogcn compounds which consists in adding thereto disintegrated chlorid of calcium and subjecting the mixture to the action of steam and heat. f

In testimony whereof I'have hereunto set my hand in presence of two Witnesses.

CONSTANTIN KRAUSS. I'Vitnesses HENRY HASPER, WOLDEMAR HAUPT. 

